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Method for preparing lignin sulfonate by utilizing papermaking black liquid

A technology of sulfonated lignin and papermaking black liquor, which is applied in the field of papermaking, can solve the problems affecting the performance of sulfonated products and the low value of sulfonated degree, so as to achieve low content of total reducing substances, reduce the generation of by-products, effective response

Active Publication Date: 2018-07-24
HAINAN JINHAI PULP & PAPER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Add FeCl to the reaction system 2 As a catalyst, it is beneficial to increase the degree of sulfonation, but the value of the degree of sulfonation is still low, which cannot meet our needs
Adding copper salt as a catalyst in the reaction system is beneficial to increase the degree of sulfonation, which is much higher than that of FeCl 2 Catalytic sulfonation experiment results, but copper salt may affect the performance of sulfonated products

Method used

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  • Method for preparing lignin sulfonate by utilizing papermaking black liquid

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Embodiment 1

[0020] A method of utilizing papermaking black liquor to prepare sulfonated lignin, comprising the following steps:

[0021] S1, material preparation: prepare sulfate pulping black liquor, anhydrous sodium sulfite, formaldehyde raw materials, the amount of sodium sulfite is 2.9mmol / g lignin; the amount of formaldehyde is 0.8mmol / g lignin, and it is formulated into a mass concentration of 30% formaldehyde solution;

[0022] S2. Reaction: First, add sulfate pulping black liquor into the 3L stainless steel high-pressure reactor, then add sodium sulfite and formaldehyde solution, close the reactor, open the stirrer, set the stirring speed to 130r / min, and electrify to heat up, gradually heat up , when the reaction temperature reaches 105°C, open the vent valve for a small vent for 1min, then close the vent valve and continue heating until the temperature in the reactor reaches 158°C, and continue to stir the reaction at this temperature for 3.5h to control the pressure in the reac...

Embodiment 2

[0027] A method of utilizing papermaking black liquor to prepare sulfonated lignin, comprising the following steps:

[0028] S1, material preparation: prepare sulfate pulping black liquor, anhydrous sodium sulfite, formaldehyde raw materials, the amount of sodium sulfite is 3.2mmol / g lignin; the amount of formaldehyde is 1.2mmol / g lignin, and it is formulated into a mass concentration of 40% formaldehyde solution;

[0029] S2. Reaction: First, add sulfate pulping black liquor into the 250L stainless steel high-pressure reactor, then add sodium sulfite and formaldehyde solution, close the reactor, open the stirrer, set the stirring speed to 170r / min, and electrify to heat up, gradually heat up , when the reaction temperature reaches 110°C, open the vent valve for a small vent for 1min, then close the vent valve and continue heating until the temperature in the reactor reaches 165°C, and continue to stir the reaction at this temperature for 2.5h; control the pressure in the reac...

Embodiment 3

[0034] A method of utilizing papermaking black liquor to prepare sulfonated lignin, comprising the following steps:

[0035] S1, material preparation: prepare sulfate pulping black liquor, anhydrous sodium sulfite, formaldehyde raw materials, the amount of sodium sulfite is 3.0mmol / g lignin; the amount of formaldehyde is 1.0mmol / g lignin, and it is formulated into a mass concentration of 37% formaldehyde solution;

[0036] S2. Reaction: firstly add sulfate pulping black liquor into the 500L stainless steel autoclave, then add sodium sulfite and formaldehyde solution, close the reactor, open the stirrer, set the stirring speed to 150r / min, and electrify to heat up, gradually heat up , when the reaction temperature reaches 105 ℃, open the vent valve for a small vent for 1min, then close the vent valve and continue heating until the temperature in the reactor reaches 160 ℃, and continue to stir the reaction at this temperature for 3.0h; control the pressure in the reactor not mo...

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Abstract

The invention discloses a method for preparing lignin sulfonate by utilizing papermaking black liquid. The method comprises the following steps: S1, preparing raw materials: preparing the raw materials such as the papermaking black liquid, anhydrous sodium sulfite and formaldehyde, wherein the use amount of the sodium sulfite is 2.9 to 3.2 mmol per gram of lignin, the use amount of the formaldehyde is 0.8 to 1.2 mmol per gram of lignin, and the formaldehyde is prepared into a formaldehyde solution; S2, performing reaction: adding the papermaking black liquid into a reaction kettle, adding thesodium sulfite and the formaldehyde solution, stirring and heating, gradually heating to 158 to 165 DEG C, and continuously stirring to perform reaction for 2.5 to 3.5 hours, wherein the consumed timein the heating process is 80 to 100 minutes and the temperature is increased by 1 to 5 DEG C per minute; and S3, discharging: cooling after the reaction, and discharging when the temperature is reduced to 60 to 70 DEG C. The lignin sulfonate prepared by the method has high sulfonation degree and excellent tainting property, dispersibility and heat-resistant stability, has low water content and low content of sulfate, calcium, magnesium, iron, water insoluble matters and total reducing matters, has excellent comprehensive quality and can be widely applied in various fields.

Description

technical field [0001] The invention relates to the technical field of papermaking black liquor, in particular to a method for preparing sulfonated lignin by utilizing papermaking black liquor. Background technique [0002] The pollution-free resource utilization of papermaking black liquor has always been a problem that plagues the development of the papermaking industry. The papermaking industry wastewater contains a large amount of lignin. Alkali lignin is a by-product of acidification extraction from pulping black liquor, but the extraction yield is only about 70%. , and the extraction process produces foul-smelling hydrogen sulfide, so the recycling of lignin is not much, most of it is incinerated, and only thermal energy is used. Due to its long natural degradation time, polluting water bodies and waste of resources, the development and utilization of lignin, a superior biological resource, is attracting attention. About 140 million tons of virgin pulp is used in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00
CPCC08H6/00
Inventor 谢勤
Owner HAINAN JINHAI PULP & PAPER
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